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Water → Ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate

HRID 82216
ノート
印刷プレビュー

反応式

HRID 82216 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[N:9][NH:10]2)=[CH:6][CH:5]=1.I[CH3:20].O>C1COCC1>[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[N:9][N:10]2[CH3:20])=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 178470796HCID 178470796、化合物

生成物 1

HCID 70847731Ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Sodium hydride (24 mg, 0.602 mmol, 60% in oil) was added to ethyl (6-chloro-1H-indazol-3-yl)acetate (Preparation 168, 120 mg, 0.502 mmol) in THF (4 mL) at 0° C. and the mixture was stirred for 30 minutes. Then iodomethane (0.09 mL, 1.508 mmol) was added. The mixture was stirred at room temperature for 30 mins then water (4 mL) was added. The mixture was evaporated in vacuo and the aqueous residue was acidified with aqueous HCl (6 M). This was extracted with ethyl acetate (10 mL) and the organic phase was dried over sodium sulphate and evaporated in vacuo to afford the title compound as a white solid in 100% yield, 150 mg.

後処理

  1. stirringThe mixture was stirred at room temperature for 30 mins
  2. customThe mixture was evaporated in vacuo
  3. extractionThis was extracted with ethyl acetate (10 mL)
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-577d074b4c464056aa9e8b64afcdfa8d
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

反応ノート

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